A rapid chromatographic procedure for the isolation and quantitation of 1-(2-Aminoethyl)-3-(2,6-dichlorophenyl) thiourea from dietary admix followed by HPLC.

An analytical procedure is described for the determination of 1-(2-aminoethyl)-3-(2,6-dichlorophenyl) thiourea in dietary admix. Because of the complex nature of the carrier matrix, sample cleanup was required prior to HPLC separation. Sample cleanup was achieved using a cation-exchange microcolumn which yield highly reproducible results. HPLC separation was accomplished using a 10 mu C18 column, monitoring the column effluent in the ultraviolet region at 254 nm. After sample cleanup, 1-(2-aminoethyl)-3-(2,6-dichlorophenyl) thiourea could be detected at levels as low as 3 ppm in dietary admix.

Microcolumn chromatographic cleanup and GLC determination of 11-methyl-16,16-dimethylprostaglandin E2 in polyethylene glycol 400 solutions.

An analytical procedure is described for the GLC determination of 11-methyl-16,16-dimethylprostaglandin E2 in aqueous polyethylene glycol 400 solutions. Because of the nature of the carrier matrix, sample cleanup was required prior to GLC separation. Separation was achieved using a diethylaminoethylcellulose microcolumn. This procedure has proven to be amenable to routine analysis.

The two-dimensional characterization of amino acids in actinomycin hydrolysates.

Actinomycins, which belong to a family of chromopeptide antibiotics, consist of a hetero-tricyclic chromophore to which are attached two pentapeptide chains either identical or different in amino acid sequence. The classification of existing actinomycins and the identification of new actinomycins are dependent on the characterization and quantitation of the amino acids present in the peptide chains. A simple, fast and highly reliable two-dimensional separation technique employing electrophoresis in a formic acid/acetic acid buffer (pH 1.9) on thin layers of microcrystalline cellulose followed by thin-layer chromatography with an n-butanol:water:glacial acetic acid (50:40:10) solvent system in a direction perpendicular to the electrophoresis was developed to separate the amino acids contained in hydrolysates of the actinomycins. The separated amino acids were identified by two parameters, the chromatographic Rf value and the electrophoretic mobility calculated relative to some standard migrating compound.

Measurement of surface color and color difference of tablet colorants by tristimulus colorimetry.

The surface color of a series of color dispersions containing from one to three FD&C or D&C dyes suspended in a sucrose syrup was examined using tristimulus colorimetry. CIE (x, y) and Hunter (a, b) chromaticity data, determined directly from an integrating sphere colorimeter or from reflectance spectra and suitable calculations, were used to order materials by color on expanded chromaticity diagrams. Color difference was evaluated quantitatively from Hunter (a, b) data using the Judd color difference formula. Quality control specifications were established either by defining areas of acceptable color by applying limits to the chromaticity coordinates of color standards or by requiring the Judd color difference to be less than a specific number of National Bureau of Standards standard units. This method eliminates the subjective character of color evaluation and permits the quantitation of visual color difference. These differences can be used, in conjunction with defined color standards, to develop color specifications for tablet colorants, finished tablets, and liquid and cream pharmaceutical preparations.